Reacción #95219

ord-8e93b465b8fa4b39bec5f67f154ba6ef

Disolventes

Condiciones de reacción

Temperatura
-10°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe crude product precipitated from the reaction mixture
  2. 2
    FiltraciónAfter isolation by filtration
  3. 3
    Lavadothe residue was washed with hot petroleum ether
  4. 4
    Otrofinally recrystallized from methylene chloride

Procedimiento

A solution of 10.9 g (0.05 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 12.6 g (0.055 mole) 3,5-dinitrobenzoyl chloride in 200 ml toluene was refluxed for 20 hours. The crude product precipitated from the reaction mixture upon cooling to -10° C. After isolation by filtration, the residue was washed with hot petroleum ether and finally recrystallized from methylene chloride to give 17.5 g (85% yield) of pure product; m.p. 197° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04343945uspto-grants-1982_08